CN111333577A - Brand-new caprolactam production system - Google Patents

Brand-new caprolactam production system Download PDF

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Publication number
CN111333577A
CN111333577A CN202010119227.3A CN202010119227A CN111333577A CN 111333577 A CN111333577 A CN 111333577A CN 202010119227 A CN202010119227 A CN 202010119227A CN 111333577 A CN111333577 A CN 111333577A
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China
Prior art keywords
discharge end
tower
tank
benzene
washing
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CN202010119227.3A
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Chinese (zh)
Inventor
谢文理
吴望成
瞿亚平
刘期敏
张泽渐
刘志强
肖高荣
张方
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Fujian Eversun Technology Co ltd
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Fujian Eversun Technology Co ltd
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Priority to CN202010119227.3A priority Critical patent/CN111333577A/en
Publication of CN111333577A publication Critical patent/CN111333577A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D223/00Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom
    • C07D223/02Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings
    • C07D223/06Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D223/08Oxygen atoms
    • C07D223/10Oxygen atoms attached in position 2
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D201/00Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/16Separation or purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a brand new caprolactam production system, which comprises a hexane extraction tower, wherein the discharge end of the hexane extraction tower is connected with a buffer tank, the discharge end of the buffer tank is connected with a benzene hexane buffer tank through a guide pipe, the discharge end of the benzene hexane buffer tank is connected with a washing tower for cleaning materials, the discharge end of the top of the washing tower is connected with a receiving tank, the discharge end of the bottom of the receiving tank is connected with a discharge pump of the receiving tank, the discharge end of the discharge pump of the receiving tank is connected with a benzene evaporation first tower, the discharge end of the bottom of the benzene distillation tower is connected with the feed end of the benzene distillation tower II, the discharge end of the benzene distillation tower II is connected with a hexane buffer tank, the discharge end of the hexane buffer tank is connected with an ion exchange tower, the discharge end of the ion exchange tower is connected with a head tank, the discharge end of the elevated tank is connected with the feed end of the reactor, so that the invention simplifies the equipment, reduces the cost, has stable finished product quality, long storage time and strong practicability.

Description

Brand-new caprolactam production system
Technical Field
The invention relates to the technical field of caprolactam generation processes, in particular to a brand-new caprolactam production system.
Background
In the existing caprolactam refining device, basic composition units are extraction → benzene evaporation recovery → an ion exchange tower → hydrogenation of a hydrogenation reactor → evaporation concentration → distillation refining, the process is complex, the labor investment is large, the equipment cost and the maintenance cost are also high, and the finished product quality of the traditional process is unstable and fluctuates frequently.
The material got into the scrubbing tower after having extracted among the traditional flow extraction process washes the back-extraction tower and carries out reverse water extraction earlier through the back-extraction tower again and retrieve the benzene in the hexane liquid through the benzene return tower, and this flow back-extraction tower extraction effect is unstable, and caprolactam is often smugglied secretly for miscellaneous benzene to the benzene that goes out at top, causes the loss of caprolactam to the back-extraction tower cost is high, and benzene recovery tower evaporates the benzene effect operation degree of difficulty higher, smugglies easily and causes the play hexane to contain benzene and exceeds standard, causes the loss of benzene.
The pre-distillation and distillation device after evaporation has large energy consumption, large occupied area, large investment and large operation difficulty of a matched hot water system.
Disclosure of Invention
The invention aims to provide a brand new caprolactam production system to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a brand new caprolactam production system comprises a hexane extraction tower, wherein the discharge end of the hexane extraction tower is connected with a buffer tank, the discharge end of the buffer tank is connected with a benzene hexane buffer tank through a guide pipe, the discharge end of the benzene hexane buffer tank is connected with a washing tower for cleaning materials, the discharge end of the top of the washing tower is connected with a receiving tank, the discharge end of the bottom of the receiving tank is connected with a discharge pump of the receiving tank, the discharge end of the discharge pump of the receiving tank is connected with a benzene distillation first tower, the discharge end of the bottom of the benzene distillation first tower is connected with the feed end of a benzene distillation second tower, the discharge end of the benzene distillation second tower is connected with a hexane buffer tank, the discharge end of the hexane buffer tank is connected with an ion exchange tower, the discharge end of the ion exchange tower is connected with a head tank, the discharge end of the head tank is connected with the feed end of a reactor, the discharge end of the reactor is connected with an evaporation assembly for evaporating materials, and the, the discharge end of the receiving tank is connected with a crystallization assembly, the discharge end of the crystallization assembly is connected with a centrifugal assembly, the discharge end of the centrifugal assembly is connected with a screw conveyor for conveying materials, the discharge end of the screw conveyor is connected with a melting tank, the discharge end of the melting tank is connected with a dewatering tower, and the discharge end of the dewatering tower is connected with a finished product pump.
As a further scheme of the invention: the discharge end at the top of the benzene distillation tower is connected with a benzene distillation tower cooler (), the discharge end of the benzene distillation tower cooler is connected with a benzene-water separator, and the discharge end of the benzene-water separator is provided with a material guide pipe used for connecting the feed end of the extraction tower.
As a further scheme of the invention: the washing liquid in the washing tower is 1-3-% wt dilute alkali liquid.
As a further scheme of the invention: the centrifuge assembly includes at least one crystallization centrifuge.
As a further scheme of the invention: the heating temperature of the melting tank was 90 ℃.
As a further scheme of the invention: the crystallizing component at least comprises a crystallizing reactor, and the discharging temperature of the crystallizing reactor is 20-30 ℃.
As a further scheme of the invention: the evaporation assembly comprises at least one evaporation tower.
As a further scheme of the invention: and the feeding end of the benzene distillation tower is connected with a benzene distillation tower preheater for preheating materials.
As a further scheme of the invention: the washing assembly in the washing tower comprises a first mixer used for mixing caustic soda and water, the discharge end of the first mixer is connected with a washing liquid tank, the discharge end of the washing liquid tank is connected with a first feeding end of the washing tower, the discharge end of the bottom of the washing tower is connected with a circulating liquid pump, the discharge end of the circulating liquid pump is connected with a second mixer used for fully mixing materials and washing liquid, and the discharge end of the second mixer is connected with a feeding end at the top of the washing tower.
Compared with the prior art, the invention has the beneficial effects that: the device contains benzene hexane benzene distillation system, and former flow is three-effect benzene rectifying column + stripping column + debenzolization tower + benzene steam condensing system, and new system only is two-effect benzene hexane benzene distillation tower and benzene steam condensing system, has simplified 30% on the flow, can practice thrift 20-30% in the investment because the reduction of equipment, and the benzene that the benzene distillation tower evaporated out is the refined benzene, need not to use directly through benzene rectifying column, can practice thrift partial steam in the aspect of the energy.
The device also comprises a crystallization system, the primary process comprises a pre-distillation process, a matched vacuum system and a pre-distillation hot water system, the device occupies large area, occupies most of the area of five layers and four layers, the device is more, the system is in vacuum operation, four-stage vacuum pumping is adopted in the pre-distillation process, five-stage vacuum pumping is adopted in the distillation process, the process is complex and complicated in operation, medium-pressure steam is adopted in energy consumption, the unit consumption is about 0.842, the production cost of the medium-pressure steam is about 150 yuan/ton, after the caprolactam crystallization process is changed, the vacuum system is omitted for micro positive pressure, a crystallization reactor, a centrifuge, a screw machine and a dehydration tower are only arranged on the device, the device is simplified greatly, 30-40% in investment and small in operation difficulty, in the aspect of energy consumption, the system uses low-pressure steam, the unit consumption is about 0.5-0.6, and the production cost is about 120 yuan/ton, can save energy consumption cost by 10-20%, and has stable finished product quality, long storage time and strong practicability in the aspect of finished product quality.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Wherein: the system comprises a hexane extraction tower 1, a buffer tank 2, a benzene hexane buffer tank 3, a washing tower 5, a receiving tank 6, a washing liquid tank 8, a benzene distillation tower I9, a benzene distillation tower cooler (10), a benzene distillation tower II 11, a benzene water separator 12, a hexane buffer tank 13, an ion exchange tower 14, an overhead tank 15, a reactor 16, an evaporation tower 17, a receiving tank 18, a crystallization reactor 19, a crystallization centrifuge 20, a screw conveyor 21, a melting tank 22 and a dehydration tower 23.
Detailed Description
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, in an embodiment of the present invention, a brand new caprolactam production system includes a hexane extraction tower 1, a discharge end of the hexane extraction tower 1 is connected to a buffer tank 2, a discharge end of the buffer tank 2 is connected to a cyclohexane buffer tank 3 through a conduit, a discharge end of the cyclohexane buffer tank 3 is connected to a washing tower 5 for cleaning a material piece, a discharge end of a top of the washing tower 5 is connected to a receiving tank 6, a discharge end of a bottom of the receiving tank 6 is connected to a receiving tank discharge pump, a discharge end of the receiving tank discharge pump is connected to a cyclohexane first tower 9, a feed end of the cyclohexane first tower 9 is connected to a cyclohexane distillation tower preheater 8 for preheating the material, a discharge end of a bottom of the cyclohexane first tower 9 is connected to a feed end of a cyclohexane second tower 11, a discharge end of the cyclohexane second tower 11 is connected to a hexane buffer tank 13, a discharge end of the hexane buffer tank 13 is connected to an ion exchange tower 14, a discharge end of the ion exchange tower 14 is connected to a high-level tank, the discharge end of the elevated tank 15 is connected with the feed end of the reactor 16, the discharge end of the reactor 16 is connected with an evaporation assembly for evaporating materials, the evaporation assembly at least comprises an evaporation tower 17, the discharge end of the evaporation assembly is connected with a receiving tank 18, the discharge end of the receiving tank 18 is connected with a crystallization assembly, the discharge end of the crystallization assembly is connected with a centrifugal assembly, the crystallization assembly comprises at least one crystallization reactor 19, the discharge temperature of the crystallization reactor 19 is 20-30 ℃, the centrifugal assembly at least comprises a crystallization centrifuge 20, the discharge end of the centrifugal assembly is connected with a screw conveyer 21 for conveying materials, the discharge end of the screw conveyer 21 is connected with a melting tank 22, the heating temperature of the melting tank 22 is 90 ℃, the discharge end of the melting tank 22 is connected with the dehydrating tower 23, and the discharge end of the dehydrating tower 23 is connected with a finished product pump;
the discharge end of the top of the benzene distillation tower 9 is connected with a benzene distillation tower cooler (10), the discharge end of the benzene distillation tower cooler 10 is connected with a benzene-water separator 12, and the discharge end of the benzene-water separator 12 is provided with a material guide pipe for connecting the feed end of the extraction tower 1;
the washing component in the washing tower 5 comprises a first mixer used for mixing caustic soda and water, the discharge end of the first mixer is connected with a washing liquid tank 8, the discharge end of the washing liquid tank 8 is connected with a first feeding end of the washing tower 5, the discharge end of the bottom of the washing tower 5 is connected with a circulating liquid pump, the discharge end of the circulating liquid pump is connected with a second mixer used for fully mixing materials and washing liquid, the discharge end of the second mixer is connected with a feeding end of the top of the washing tower 5, the washing liquid in the washing tower 5 is 1-3% wt dilute alkali liquid, and the materials and the washing liquid in the washing tower are fully mixed under the action of the circulating liquid pump, so that the materials are washed.
The working principle of the invention is as follows: the process is communicated from front to back, materials enter an extraction tower 1 in a front process to form benzene hexane liquid with the concentration of about 18-24% by weight, enter a buffer tank 2, are washed by 1-3% by weight of dilute alkali liquor in a washing tower 5, enter the top of a benzene hexane distillation benzene first tower 9 to separate benzene into refined benzene, less impurities can be directly returned to the extraction tower for use, bottom layer liquid in a tower bottom enters a benzene hexane distillation benzene second tower 11 to be debenzolized, the benzene content is less than 50ppm, the refined benzene enters a hexane buffer tank 13 to pass through an ion exchange tower 14, an overhead tank 15, a reactor 16 and an evaporation first tower/second tower/third tower 17 to concentrate the concentration to 90% and then enters a caprolactam crystallization system, the caprolactam crystallization system is cooled to 20-30 ℃ through a crystallization reactor 19, the liquid caprolactam can separate out crystals in the crystallization reactor 19 to form crystal slurry, and then enters a crystallization centrifuge 20 to centrifugally separate caprolactam solid with the water content of about 0.5% through gravity action, conveyed to a melting tank 22 by a screw conveyor 21, heated to 90 ℃ by a steam jacket to become a molten state, and enters a dehydration tower 23 to be dehydrated into a final caprolactam finished product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. A brand new caprolactam production system comprises a stripping tower (1) and is characterized in that the discharge end of the stripping tower (1) is connected with a buffer tank (2), the discharge end of the buffer tank (2) is connected with a benzene hexane buffer tank (3) through a guide pipe, the discharge end of the benzene hexane buffer tank (3) is connected with a washing tower (5) used for cleaning materials, the discharge end of the top of the washing tower (5) is connected with a receiving tank (6), the discharge end of the bottom of the receiving tank (6) is connected with a receiving tank discharge pump, the discharge end of the receiving tank discharge pump is connected with a benzene distillation tower (9), the discharge end of the bottom of the benzene distillation tower (9) is connected with the feed end of a benzene distillation tower (11), the discharge end of the benzene distillation tower (11) is connected with a hexane buffer tank (13), the discharge end of the hexane buffer tank (13) is connected with an ion exchange tower (14), and the discharge end of the ion exchange tower (14) is connected with a head tank (15), the discharge end of elevated tank (15) is connected with the feed end of reactor (16), the discharge end of reactor (16) is connected and is used for carrying out evaporation treatment's evaporation subassembly to the material, and evaporation subassembly's discharge end is connected and is received jar (18), the discharge end of receiving jar (18) is connected the crystallization subassembly, and centrifugal subassembly is connected to the discharge end of crystallization subassembly, screw conveyor (21) that are used for carrying the material are connected to the discharge end of centrifugal subassembly, and melting tank (22) is connected to the discharge end of screw conveyor (21), dehydration tower (23) is connected to the discharge end of melting tank (22), the finished product pump is connected to the discharge end of dehydration tower (23).
2. The brand new caprolactam production system according to claim 1, wherein a discharge end of the top of the benzene distillation tower (9) is connected with a benzene distillation tower cooler (10), a discharge end of the benzene distillation tower cooler (10) is connected with a benzene water separator (12), and a discharge end of the benzene water separator (12) is provided with a material guide pipe for connecting with a feed end of the extraction tower (1).
3. A brand new caprolactam production system according to claim 1, characterized in that the washing liquid in the washing column (5) is 1-3% wt dilute lye.
4. Brand new caprolactam production system according to claim 1, wherein said centrifugation means comprise at least one crystallization centrifuge (20).
5. A brand new caprolactam production system according to claim 1, characterized in that the heating temperature of the melting tank (22) is 90 ℃.
6. A brand new caprolactam production system according to claim 1, characterized in that said crystallization unit comprises at least one crystallization reactor (19), the discharge temperature of the crystallization reactor (19) being 20-30 ℃.
7. Brand new caprolactam production system according to claim 1, wherein said evaporation assembly comprises at least one evaporation tower (17).
8. A brand new caprolactam production system according to claim 1, characterized in that the feed end of said benzene distillation column (9) is connected to a benzene distillation column preheater 8 for preheating the material.
9. A brand new caprolactam production system according to claim 1, wherein the washing assembly in the washing column (5) comprises a first mixer for mixing caustic soda and water, the discharge end of the first mixer is connected with a washing liquid tank (8), the discharge end of the washing liquid tank (8) is connected with a first feed end of the washing column (5), the discharge end of the bottom of the washing column (5) is connected with a circulating liquid pump, the discharge end of the circulating liquid pump is connected with a second mixer for thoroughly mixing the material and the washing liquid, and the discharge end of the second mixer is connected with a feed end of the top of the washing column (5).
CN202010119227.3A 2020-02-26 2020-02-26 Brand-new caprolactam production system Pending CN111333577A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000066561A1 (en) * 1999-04-29 2000-11-09 Dsm N.V. Process for the preparation of caprolactam
CN1323786A (en) * 2001-04-12 2001-11-28 巨化集团公司 Technology for extracting caprolactam and direct steam debenzolization
CN105622510A (en) * 2014-11-04 2016-06-01 中国石油化工股份有限公司 Refining method of caprolactam
CN107556240A (en) * 2016-08-24 2018-01-09 沧州旭阳化工有限公司 A kind of system of caprolactam refining method and refined caprolactam
CN109665998A (en) * 2017-10-17 2019-04-23 中国石油化工股份有限公司 The refining methd and device of caprolactam
CN110668910A (en) * 2019-09-23 2020-01-10 聊城煤泗新材料科技有限公司 Benzene distillation residue recovery device, recovery method and application
CN110804018A (en) * 2019-12-11 2020-02-18 河北美邦工程科技股份有限公司 Refining method and refining system of caprolactam

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000066561A1 (en) * 1999-04-29 2000-11-09 Dsm N.V. Process for the preparation of caprolactam
CN1323786A (en) * 2001-04-12 2001-11-28 巨化集团公司 Technology for extracting caprolactam and direct steam debenzolization
CN105622510A (en) * 2014-11-04 2016-06-01 中国石油化工股份有限公司 Refining method of caprolactam
CN107556240A (en) * 2016-08-24 2018-01-09 沧州旭阳化工有限公司 A kind of system of caprolactam refining method and refined caprolactam
CN109665998A (en) * 2017-10-17 2019-04-23 中国石油化工股份有限公司 The refining methd and device of caprolactam
CN110668910A (en) * 2019-09-23 2020-01-10 聊城煤泗新材料科技有限公司 Benzene distillation residue recovery device, recovery method and application
CN110804018A (en) * 2019-12-11 2020-02-18 河北美邦工程科技股份有限公司 Refining method and refining system of caprolactam

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